Metal organic frame/graphene carried palladium nano-composite catalyst and preparing method and application thereof

A metal-organic framework and composite catalyst technology, applied in the field of catalysis, to achieve the effects of simple preparation process, easy industrialization, and excellent carrier characteristics

Active Publication Date: 2016-02-24
新疆申基生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports on graphene/organometallic framework composites sup

Method used

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  • Metal organic frame/graphene carried palladium nano-composite catalyst and preparing method and application thereof
  • Metal organic frame/graphene carried palladium nano-composite catalyst and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation method of graphene oxide:

[0020] Take graphite powder and sodium nitrate, add concentrated sulfuric acid and stir evenly, then put it in an ice bath, add potassium permanganate while stirring, keep the temperature below 20℃, then heat up to 35℃ and keep it for 1~2h, add slowly Ionized water, the volume ratio of the added deionized water and concentrated sulfuric acid is 2:1, and the temperature is increased to 85~95℃, kept for 15min, then add 10mL30% hydrogen peroxide and deionized water, the deionized water added at this time The volume ratio of water to concentrated sulfuric acid is 6:1. The resulting product is centrifuged, washed with dilute hydrochloric acid, dried, and ground to obtain graphene oxide; the mass ratio of graphite powder to sodium nitrate is 2:1, concentrated sulfuric acid to graphite The powder ratio is 23mL / mg, and the mass ratio of potassium permanganate to graphite powder is 3:1.

[0021] (2) Preparation method of metal organic fram...

Embodiment 2

[0025] (1) The preparation method of graphene oxide is the same as in Example 1;

[0026] (2) Preparation method of metal organic framework / graphene supported palladium nano composite catalyst:

[0027] Weigh 100mg of the graphene oxide prepared above and put it into a beaker, add 10mL DMF, ultrasonically disperse for 60min, and add 1.0g ZrCl to it in turn 4 , 712mg terephthalic acid and 200mL DMF, the resulting solution was slowly stirred at 120°C for 18h, allowed to stand, filtered, and the filter cake was washed with DMF. The crude product was immersed in dichloromethane for 12h, filtered with suction, and dried overnight at room temperature under vacuum. In an oven at 100°C and a constant temperature for 12 hours, the composite UiO66GO is finally obtained.

[0028] Disperse 200mg UiO66GO composite material in n-hexane and ultrasonic for 30min to form a quasi-homogeneous system. While stirring, add 2mL dropwise to a concentration of 0.04mol / LH 2 PdCl 4 The solution, continue to s...

Embodiment 3

[0030] (1) The preparation method of graphene oxide is the same as in Example 1;

[0031] (2) Preparation method of metal organic framework / graphene supported palladium nano composite catalyst:

[0032] Weigh 100mg of the graphene oxide prepared above and put it into a beaker, add 10mL DMF, ultrasonically disperse for 100min, and add 2.5g ZrCl to it in turn 4 , 1.8g terephthalic acid and 500mL DMF, the resulting solution was slowly stirred at 120°C for 24h, allowed to stand, filtered, and the filter cake was washed with DMF. The crude product was immersed in dichloromethane for 24h, filtered with suction, and dried at room temperature under vacuum overnight. In an oven at 120°C and a constant temperature for 24 hours, the composite material UiO66GO is finally obtained.

[0033] Disperse 200mg UiO66GO composite material in n-hexane and ultrasonic for 30min to form a quasi-homogeneous system. Under stirring, add 0.8mL dropwise to a concentration of 0.04mol / LH 2 PdCl 4 Solution, contin...

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Abstract

The invention discloses a metal organic frame/graphene carried palladium nano-composite catalyst and a preparing method and application thereof. Firstly, anhydrous zirconium tetrachloride, terephthalic acid and N,N-diamide are added in a graphene oxide solution to prepare a metal organic frame/graphene composite; secondly, normal hexane, an H2PdCl4 solution and a reducing agent are added to obtain the metal organic frame/graphene carried palladium nano-composite catalyst, wherein a carrier of the catalyst is composed of the metal organic frame and graphene, palladium nano-particles serve as carried active components, the carrying quantity of the palladium nano-particles accounts for 1-10% of the total mass of the catalyst, and the particle size ranges from 10 nm to 20 nm. The metal organic frame/graphene carried palladium nano-composite catalyst shows high catalytic activity and good reuse performance when applied to a Suzuki reaction of halogeno benzene and phenylboronic acid.

Description

Technical field [0001] The invention relates to a catalyst, in particular to a metal organic framework / graphene loaded palladium nano composite catalyst and a preparation method and application thereof, belonging to the technical field of catalysis. Background technique [0002] Since 2004, graphene (GN) has been widely studied by scholars at home and abroad as a new type of carbon nanomaterial. The ultra-high specific surface, good conductivity and mechanical strength make graphene a catalyst support material with good potential and excellent performance. Achieving high-quality dispersion and loading of precious metal nanoparticles on the surface of graphene has always been a topic worthy of attention. However, since graphene has a large conjugated system, the strong π-π interaction between the layers is prone to superimposition, which will cause greater interference to the dispersion and stability of precious metal nanoparticles. How to more effectively combine precious metal...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10C07C15/14C07C1/32
Inventor 刘想赵晓华朱建军石秋忠徐吉成陆道明
Owner 新疆申基生物科技有限公司
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